EP1103526A2 - Matière active pour générateurs électrochimiques rechargeables - Google Patents

Matière active pour générateurs électrochimiques rechargeables Download PDF

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Publication number
EP1103526A2
EP1103526A2 EP00124313A EP00124313A EP1103526A2 EP 1103526 A2 EP1103526 A2 EP 1103526A2 EP 00124313 A EP00124313 A EP 00124313A EP 00124313 A EP00124313 A EP 00124313A EP 1103526 A2 EP1103526 A2 EP 1103526A2
Authority
EP
European Patent Office
Prior art keywords
hydroxide
mixed
nickel
metal
mixed metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00124313A
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German (de)
English (en)
Other versions
EP1103526A3 (fr
Inventor
Oskar Prof. Dr. Glemser
Sven Dr. Albrecht
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toda Kogyo Europe GmbH
Original Assignee
HC Starck GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HC Starck GmbH filed Critical HC Starck GmbH
Publication of EP1103526A2 publication Critical patent/EP1103526A2/fr
Publication of EP1103526A3 publication Critical patent/EP1103526A3/fr
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/02—Carbonyls
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to an active material for rechargeable batteries, especially a metal (III) ion-substituted nickel hydroxide with a brucite-like structure, a process for its production and its use as an electrode material for secondary batteries.
  • the ⁇ -structure succeeds (Pyroaurite) stabilize.
  • the pyroaurite structure Ensuring charge neutrality between anions and water molecules between the nickel hydroxide layers, so that the grid is expanded.
  • the storage density is due to the electrovalent 3valent ones Ions and on the other hand through the embedded anions and water molecules reduced.
  • the 3-valent suspension can be used Ion modified pyroaurite nickel hydroxide in alkali solution, separation from the Alkali solution and drying with the still attached alkali solution the pyroaurite structure into a brucite-like structure while maintaining the 1.67 electron step convict. Interlayer anions and water are removed from the grid, so that the layer spacing is reduced while increasing the storage density.
  • the present invention accordingly relates to a mixed metal hydroxide Brucite structure, the nickel hydroxide as the main component and at least one Trivalent metal from the group Co, Fe, Al, Ga, In, Sc, Y and La in one quantity from 12 to 30 atomic% based on the sum of the metal components inclusive Contains nickel.
  • the trivalent metal is preferably present in an amount of 12 to 25 atom% on the sum of all metal components available.
  • Preferred trivalent metals are Co, Fe and Al, particularly preferably Al.
  • Particularly preferred mixed metal hydroxides according to the invention with a brucite structure contain at least in addition to the above-mentioned first group of trivalent metals one of the elements Co, Fe, Mn, Cr, Ti, Zr and Cu, the element being these second group from the trivalent metal of the first group and that Trivalent metal of the first group substituted in an amount of up to 40 atom%.
  • Preferred mixed metal hydroxides according to the invention contain Al and Co, wherein the atomic ratio of Al to Co is 2 to 4, particularly preferably 2.5 to 3.5.
  • the mixed metal hydroxides according to the invention are further characterized by a X-ray diffraction determined layer spacing of 4.3 to 4.8 ⁇ .
  • the reflex is to a smaller ⁇ angle by a shoulder that has a grid spacing of 5.2 to Equals 5.7 ⁇ , broadened.
  • the invention also relates to a method for producing the inventive Mixed hydroxides by co-precipitation of mixed hydroxides with pyroaurite structure from corresponding metal salt solutions, suspension of the precipitate in alkali solution, separation from the alkali solution and drying in Presence of the attached alkali solution.
  • An at least 0.5 molar alkali hydroxide solution is preferably used.
  • At least 0.9 molar alkali hydroxide solution is used for the alkaline drying, particularly preferably an at least 1 molar alkali hydroxide solution used.
  • the preferred alkali hydroxide is sodium hydroxide.
  • the mixed hydroxides with pyroaurite structure are produced by manufacturing an aqueous solution by dissolving appropriate water-soluble metal salts the metal components in the desired ratio and precipitation from the solution by adjusting the pH to 10 to 13 by adding alkali hydroxide solutions.
  • the process can be carried out batchwise or continuously by simultaneous Feed the metal salt solution and the alkali hydroxide solution to a reaction container with continuous deduction of the precipitation suspension.
  • Metal salts are suitable halides (preferably fluorides or chlorides), Carbonates, sulfates, nitrates, acetates, oxalates, borates and / or phosphates, to the extent these have sufficient solubility.
  • oxidizing agents such as, for example, oxygen, H 2 O 2 , hypochlorite or peroxodisulfates.
  • Alkali solutions for carrying out the precipitation are ammonium hydroxide, Lithium hydroxide, potassium hydroxide or sodium hydroxide in question. Is preferred Sodium hydroxide.
  • the precipitation may be mixed into the mixed metal hydroxide built-in anions of the pyroaurite structure initially through carbonate ions exchange. This can be done by treating the precipitate with alkali carbonate or alkali hydrogen carbonate solution.
  • the precipitate becomes after separation from the mother liquor and washing Removal of residual mother liquor preferably without intermediate drying in an alkali hydroxide solution.
  • After separation from the alkali hydroxide solution be careful at temperatures below 80 ° C, especially below 60 ° C, more preferably dried under reduced pressure.
  • the lower the Pressure chosen during drying, the higher the minimum should be Concentration of the alkali hydroxide solution. For example, one Drying pressure of 10 mbar an alkali hydroxide concentration of at least 1.3 molar preferred.
  • the mixed metal hydroxides with brucite structure obtainable according to the invention are at the same time, excellent raw materials for the production of lithium mixed metal oxides.
  • the lithium mixed metal oxides are produced in that the mixed metal hydroxides with suitable lithium compounds such as lithium hydroxide or lithium nitrate are mixed and then the mixture Temperatures above 600 ° C are burned.
  • Fig. 1 explains in an idealized representation that with the different nickel hydroxides achievable electron transitions.
  • the top four structures show the well-known Bode diagram.
  • Fig. 3 shows the discharge capacity of the mixed hydroxide of the brucite type depending the number of cycles according to the following example.
  • the coprecipitation of the substituted nickel hydroxides takes place by dropping the mixed metal salt solution into a template of constant pH.
  • the composition of the metal salt solution, the equalizing solution and the initial charge is described here for the example of a precipitation of 0.125 mol of a nickel hydroxide of the metal ion composition Ni 4 Al 0.75 Co 0.25 at a precipitation pH of 12.5.
  • the composition of the metal salt solution is changed accordingly. With this batch size, about 10 g of dried hydroxide are obtained. 1.
  • the template is thermostated to a temperature of 34 ° C before precipitation. During the precipitation the pH is measured and by varying the The addition speed of the compensating liquor was kept constant. The stirring speed during the precipitation is 300 rpm.
  • the saline solution is pumped at a rate of 5 ml / minute with membrane pumps added to the template and the pH value by adding the equalizing solution kept constant at 12.5.
  • the precipitate is centrifuged off at 6000 rpm for 10 minutes, the supernatant Discarded lye and the product with a mixer in a liter of wash liquor (NaOH) from the precipitation pH at room temperature for about 3 minutes and then centrifuged again. This process is repeated until the one to be washed out Anion is no longer detectable.
  • the washed gel is suspended in 200 ml of one Sodium hydroxide solution of a certain concentration according to Table 1, stirs Hour, centrifuged and dried with the adhesive alkali at 50 ° C in a water jet vacuum.
  • This process is referred to here as alkaline drying.
  • In the degree of conversion decreases with the hydroxide ion concentration of the products used suspension liquor to (Fig. 2).
  • a pyroaurite type from 0.4 molar lye becomes one Preserved spectrum with low levels of brucite.
  • drying from 0.7 molar Lye is almost completely converted to the brucite type.
  • the ratio of This treatment does not change metal ions to each other. It comes off So no aluminum out of the substance due to the alkaline drying.
  • the brucite type obtained differs from the classic brucite type in that that the 001 reflex shifted somewhat to smaller d values of 4.56 ⁇ instead of 4.63 ⁇ is.
  • the 001 peak is 4.63 ⁇ and there is no shoulder at higher d values.
  • Ni 4 Al 0.75 Co 0.25 hydroxides increases with increasing proportion of the brucite structure (Table 1), as does the pycnometric density.
  • the hydroxide layers have a positive charge due to the partial substitution with trivalent cations (Al 3+ , Co 3+ or Fe 3+ ). Due to the necessary charge balancing by carbonate ions or other anions, the distance between the hydroxide layers has widened to 7.8 ⁇ . In addition, there are water molecules in the intermediate layer. In order to bring about a transformation into the brucite structure, the positive charge of the hydroxide layers must be removed.
  • the completely converted product (drying from 1.0M NaOH) has a pycnometric density of 3.21 g / cm 3 .
  • a pure nickel (II) hydroxide which was produced according to the same precipitation parameters, has a pycnometric density of 3.57 g / cm 3 . If one replaces in this pure nickel hydroxide according to the formula Ni 4 Al 0.75 Co 0.25 17.65% of the nickel ions with the lighter aluminum ions, one obtains a density of 3.23 g / cm 3 in good agreement with the measured one Value of 3.21 g / cm 3 .
  • Galvanostatic charges and discharges were carried out to check the electrochemical properties. 10 M KOH was used as the electrolyte. 100 mg of the active material were mixed with 50 mg graphite and 3 mg PTFE powder, triturated to a dry paste and worked into nickel foam. The formation took place 14h at 5mA, the other charges 12h at the same current. Discharging was carried out with a current of 2.5 mA up to a final discharge voltage of 0.9 V vs. Cd / Cd (OH) 2 or 0V vs. Hg / HgO. When the Ni 4 Al 0.75 Co 0.25 -brucite produced by drying from 0.7 M NaOH is cycled in 10 M KOH, the maximum nickel utilization is over 147%. This corresponds to a maximum mass-related capacity of 313 m Ah / g (FIG. 2). The nickel content of this material is 46.7%.
  • the maximum nickel utilization of the Ni 4 Al 0.75 Co 0.25 brucite type with 147% is similar to that for a Ni 4 Al 0.75 Co 0.25 pyroaurite with 144%. However, since the nickel content of the brucite type with 46.7% is 6.1% higher than for the pyroaurite type with 44.0%, its mass-related capacity with 310 mAh / g is also higher than with the pyroaurite type with 290 mAh / g.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP00124313A 1999-11-29 2000-11-16 Matière active pour générateurs électrochimiques rechargeables Withdrawn EP1103526A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19957456 1999-11-29
DE19957456A DE19957456A1 (de) 1999-11-29 1999-11-29 Aktivmaterial für wiederaufladbare Batterien

Publications (2)

Publication Number Publication Date
EP1103526A2 true EP1103526A2 (fr) 2001-05-30
EP1103526A3 EP1103526A3 (fr) 2003-10-08

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Family Applications (1)

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EP00124313A Withdrawn EP1103526A3 (fr) 1999-11-29 2000-11-16 Matière active pour générateurs électrochimiques rechargeables

Country Status (10)

Country Link
US (1) US6958139B1 (fr)
EP (1) EP1103526A3 (fr)
JP (1) JP5023408B2 (fr)
KR (1) KR100640108B1 (fr)
CN (1) CN1298211B (fr)
BR (1) BR0005624A (fr)
CA (1) CA2326935C (fr)
DE (1) DE19957456A1 (fr)
SG (1) SG83823A1 (fr)
TW (1) TW583141B (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003004418A1 (fr) * 2001-07-06 2003-01-16 H.C. Starck Gmbh Hydroxyde de nickel et procede permettant de le produire
US6740451B2 (en) 2001-12-20 2004-05-25 The Gillette Company Gold additive for a cathode including nickel oxyhydroxide for an alkaline battery
WO2002052664A3 (fr) * 2000-06-23 2004-12-23 Millenium Energy Llc Nouvelles compositions destinees a etre utilisees dans des accumulateurs, des condensateurs, des cellules electrochimiques et des dispositifs similaires et pour produire de l'hydrogene
EP2289851A1 (fr) 2002-03-04 2011-03-02 The Gillette Company Fabrication d'oxyhydroxyde de nickel au moyen d'ozone
EP1805834A4 (fr) * 2004-09-24 2011-03-02 Lg Chemical Ltd Precurseur composite pour oxyde metallique a transition lithium contenant de l'aluminium et procede de preparation correspondant

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004044557B3 (de) * 2004-09-15 2006-06-14 Bayer Inc., Sarnia Mischmetallhydroxide, deren Herstellung und Verwendung
CA2751819C (fr) 2009-02-20 2013-12-10 Umicore Materiaux d'electrode positive non homogenes combinant une haute securite et une forte puissance dans une batterie rechargeable au lithium
EP2421077B1 (fr) 2010-08-17 2013-10-23 Umicore Matériaux d' électrode positive combinant une haute sécurité et haute puissance dans une batterie Li rechargeable

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DE3520108A1 (de) * 1985-06-05 1986-12-11 Varta Batterie Ag, 3000 Hannover Positive sammlerelektrode fuer akkumulatoren mit alkalischem elektrolyten
US5700596A (en) * 1991-07-08 1997-12-23 Matsushita Electric Industrial Co., Ltd. Nickel hydroxide active material powder and nickel positive electrode and alkali storage battery using them
JP3239410B2 (ja) * 1991-12-28 2001-12-17 株式会社ユアサコーポレーション アルカリ蓄電池用ニッケル電極とこれを用いたアルカリ蓄電池
US5523182A (en) * 1992-11-12 1996-06-04 Ovonic Battery Company, Inc. Enhanced nickel hydroxide positive electrode materials for alkaline rechargeable electrochemical cells
DE4323007C2 (de) * 1993-07-09 1995-06-08 Starck H C Gmbh Co Kg Mangan(III)-haltiges Nickel(II)-hydroxid, ein Verfahren zu seiner Herstellung sowie seine Verwendung als Elektrodenmaterial für Sekundärbatterien
JPH07201324A (ja) * 1993-12-29 1995-08-04 Furukawa Electric Co Ltd:The ニッケル極用水酸化ニッケルの製造方法、およびその水酸化ニッケルを用いたニッケル極、ならびにそれを組込んだアルカリ二次電池
DE69505911T2 (de) 1994-08-04 1999-04-08 Sanyo Electric Co., Ltd., Moriguchi, Osaka Aktivmasse Pulver für nichtgesinterte Nickelelektrode, nichtgesinterte Nickelelektrode für alkalische Batterie und Verfahren zu ihrer Herstellung
DE4439989C2 (de) * 1994-11-09 1997-06-19 Starck H C Gmbh Co Kg Mangan-haltige Nickel(II)-hydroxid-Pulver, Verfahren zu ihrer Herstellung sowie deren Verwendung
EP0801431A4 (fr) * 1995-11-22 1999-02-24 Matsushita Electric Industrial Co Ltd Materiau actif a base d'hydroxyde de nickel pour batterie alcaline de stockage et plaque positive
JPH09237630A (ja) * 1996-02-29 1997-09-09 Matsushita Electric Ind Co Ltd アルカリ蓄電池用活物質および正極
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JPH10125318A (ja) * 1996-10-24 1998-05-15 Matsushita Electric Ind Co Ltd アルカリ蓄電池用正極活物質および正極
KR100205136B1 (ko) * 1996-12-13 1999-07-01 손욱 니켈 계열 전지의 양극용 활물질 및 이의 제조 방법
JP3191752B2 (ja) * 1996-12-26 2001-07-23 松下電器産業株式会社 ニッケル−水素二次電池およびその電極の製造方法
JP4051771B2 (ja) * 1997-06-10 2008-02-27 堺化学工業株式会社 水酸化ニッケル粒子、その製造方法、これを原料とするリチウム・ニッケル複合酸化物粒子及びその製造方法
JP3449176B2 (ja) * 1997-07-01 2003-09-22 松下電器産業株式会社 アルカリ二次電池用正極活物質の製造方法
EP1044927B1 (fr) * 1998-06-10 2012-07-25 Sakai Chemical Industry Co., Ltd. Particules d'hydroxyde de nickel, leur production, et leur utilisation
JP2002524832A (ja) * 1998-09-04 2002-08-06 エバーセル・インク 電気化学セル用水酸化ニッケル活性物質
US6576368B1 (en) * 1998-10-02 2003-06-10 Sanyo Electric Co., Ltd. Positive active material for use in sealed alkaline storage batteries
US6193871B1 (en) * 1998-12-09 2001-02-27 Eagle-Picher Industries, Inc. Process of forming a nickel electrode

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002052664A3 (fr) * 2000-06-23 2004-12-23 Millenium Energy Llc Nouvelles compositions destinees a etre utilisees dans des accumulateurs, des condensateurs, des cellules electrochimiques et des dispositifs similaires et pour produire de l'hydrogene
WO2003004418A1 (fr) * 2001-07-06 2003-01-16 H.C. Starck Gmbh Hydroxyde de nickel et procede permettant de le produire
KR100856589B1 (ko) * 2001-07-06 2008-09-03 하.체. 스타르크 게엠베하 수산화니켈 및 그의 제조 방법
US7563431B2 (en) 2001-07-06 2009-07-21 H. C. Starck Gmbh Nickel hydroxide and method for producing same
US6740451B2 (en) 2001-12-20 2004-05-25 The Gillette Company Gold additive for a cathode including nickel oxyhydroxide for an alkaline battery
EP2289851A1 (fr) 2002-03-04 2011-03-02 The Gillette Company Fabrication d'oxyhydroxyde de nickel au moyen d'ozone
EP1805834A4 (fr) * 2004-09-24 2011-03-02 Lg Chemical Ltd Precurseur composite pour oxyde metallique a transition lithium contenant de l'aluminium et procede de preparation correspondant
US8216676B2 (en) 2004-09-24 2012-07-10 Lg Chem, Ltd. Composite precursor for aluminum-containing lithium transition metal oxide and process for preparation of the same

Also Published As

Publication number Publication date
SG83823A1 (en) 2001-10-16
KR100640108B1 (ko) 2006-10-31
EP1103526A3 (fr) 2003-10-08
JP5023408B2 (ja) 2012-09-12
JP2001189153A (ja) 2001-07-10
BR0005624A (pt) 2001-07-10
CN1298211A (zh) 2001-06-06
CN1298211B (zh) 2011-11-02
TW583141B (en) 2004-04-11
DE19957456A1 (de) 2001-05-31
KR20010061978A (ko) 2001-07-07
CA2326935C (fr) 2010-01-19
US6958139B1 (en) 2005-10-25
CA2326935A1 (fr) 2001-05-29

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